HRID220160

反应详情

EQUATION

反应方程式

HRID 220160 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Hydrazine hydrate (5 mL) was added to a solution of Example 93C (1.07 g, 2.96 mmol) in dioxane (10 mL). The resulting solution was refluxed for 3 hours before it was cooled and partitioned with tetrahydrofuran and brine. The aqueous phase was acidified with 6 N hydrochloric acid to pH 2 and extracted repeatedly with a tetrahydrofuran/ethyl acetate mixture. The combined organic phases were dried (magnesium sulfate), filtered, and concentrated. The crude product was recrystallized from ethyl acetate and hexane to provide a light brown solid.

WORKUP

后处理

  1. temperatureThe resulting solution was refluxed for 3 hours before it
  2. temperaturewas cooled
  3. custompartitioned with tetrahydrofuran and brine
  4. extractionextracted repeatedly with a tetrahydrofuran/ethyl acetate mixture
  5. dry with materialThe combined organic phases were dried (magnesium sulfate)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe crude product was recrystallized from ethyl acetate and hexane
  9. customto provide a light brown solid